堿性木糖醇體系回收廢鉛蓄電池鉛膏的研究
發(fā)布時(shí)間：2018-08-08 14:46
【摘要】：人類社會(huì)對(duì)鉛需求不斷增長(zhǎng),但鉛精礦產(chǎn)資源日益減少,因此回收再生鉛成為鉛工業(yè)可持續(xù)發(fā)展的一條重要途徑。同時(shí)廢鉛蓄電池若不加以合理回收,將會(huì)對(duì)環(huán)境造成很大威脅。鉛膏作為廢鉛蓄電池的重要組成部分,因其成分復(fù)雜而成為回收的重點(diǎn)和難點(diǎn)。傳統(tǒng)火法回收能耗大,鉛回收率低,產(chǎn)生的鉛塵和SO2,對(duì)環(huán)境威脅較嚴(yán)重。而濕法處理工藝由于金屬直收率高、低污染等優(yōu)點(diǎn)而日益引起了人們的關(guān)注。這其中有機(jī)物處理體系以其低污染的優(yōu)勢(shì)成為一個(gè)重要的研究方向。論文首先分別采用兩種還原劑FeSO_4和Na_2SO_3對(duì)PbO_2進(jìn)行還原轉(zhuǎn)化,采用兩種脫硫劑NaOH和Na_2CO_3對(duì)PbSO_4進(jìn)行脫硫;其次考察了鉛膏的主要組分PbO_2和PbSO_4在堿性木糖醇體系的浸出行為,并對(duì)鉛膏在堿性木糖醇體系的浸出行為進(jìn)行了研究;最后對(duì)堿性木糖醇鉛溶液的電積工藝進(jìn)行初步探索。利用X射線衍射(XRD)、掃描電鏡(SEM)、能譜(EDAX)等手段分析了反應(yīng)過(guò)程中不溶物的物相、元素組成和形貌的演變,采用傅里葉變換紅外光譜(FTIR)分析了浸出液中有機(jī)基團(tuán)的變化。本論文的主要研究成果如下:PbO_2的還原實(shí)驗(yàn)結(jié)果表明,Na_2SO_3的還原效果明顯優(yōu)于FeSO_4。FeSO_4還原最佳條件為:FeSO_4過(guò)量系數(shù)為1~1.1,反應(yīng)時(shí)間90~120min,反應(yīng)溫度90℃,H_2SO_4與PbO_2的摩爾比為3:1,但PbO_2還原率最高僅為52.4%。Na_2SO_3還原最佳條件:Na_2SO_3過(guò)量系數(shù)為6.0,反應(yīng)時(shí)間為90~120min,反應(yīng)溫度為90℃時(shí),PbO_2的還原率可達(dá)到100%。PbSO_4的脫硫轉(zhuǎn)化實(shí)驗(yàn)結(jié)果表明,NaOH脫硫的最佳條件:時(shí)間60~120min,溫度90℃,過(guò)量系數(shù)1.4,脫硫率僅為88.88%。Na_2CO_3脫硫的最佳條件:時(shí)間60~90min,溫度90℃,過(guò)量系數(shù)1.3,脫硫率僅為80.61%。紅外光譜分析結(jié)果表明,在堿性木糖醇溶液中PbO_2可以將木糖醇中的-OH氧化成-COO-,在溶液中與Pb以金屬有機(jī)化合物的形式存在。木糖醇濃度、NaOH濃度對(duì)PbO_2浸出率影響很大。PbO_2浸出率會(huì)隨著木糖醇濃度的增加呈現(xiàn)先增大后減小再增大的趨勢(shì)。木糖醇濃度的變化會(huì)導(dǎo)致PbO_2不同的溶解機(jī)制。堿性木糖醇體系PbO_2浸出的最佳條件:NaOH濃度1.5~2mol/L,木糖醇濃度為0.53~0.79mol/L,浸出溫度70℃,浸出時(shí)間30~60min,PbO_2浸出率可達(dá)99.18%。PbSO_4在堿性木糖醇體系中的浸出研究表明,木糖醇、NaOH濃度對(duì)PbSO_4的溶解量影響最大,時(shí)間和溫度影響較小。溶液中僅存在木糖醇組分時(shí),PbSO_4不會(huì)與其發(fā)生反應(yīng)。PbSO_4在堿性木糖醇體系中的溶解是在木糖醇和NaOH共同作用下完成的。PbSO_4在堿性木糖醇體系浸出的最佳條件:反應(yīng)時(shí)間60~90min,反應(yīng)溫度90℃,木糖醇濃度50~80g/L,NaOH濃度60~80g/L,PbSO_4的浸出率可達(dá)100%。對(duì)鉛膏在堿性木糖醇體系中進(jìn)行了直接浸出研究,得出鉛膏浸出的最佳條件:反應(yīng)時(shí)間30~60min,反應(yīng)溫度90℃,木糖醇濃度80~120g/L,NaOH濃度60~80g/L。鉛膏在堿性木糖醇體系的浸出率可達(dá)96.24%,在該體系下可實(shí)現(xiàn)鉛膏的短流程浸出。對(duì)堿性木糖醇體系含鉛溶液進(jìn)行電沉積的初步研究發(fā)現(xiàn):當(dāng)電流密度為140A/m~2,溫度40℃,NaOH濃度100g/L,木糖醇濃度120g/L,溶液鉛濃度100g/L,極距4cm,電解液循環(huán)速度15m L/min條件下時(shí),電流效率可達(dá)99.68%,陰極能耗為381.71k Wh/t,生成的陰極鉛表面相對(duì)平整,枝晶較少。
[Abstract]:The demand for lead is increasing in human society, but the mineral resources of lead concentrate are decreasing. Therefore, the recycling of lead has become an important way for the sustainable development of lead industry. At the same time, if the waste lead battery is not reasonably recovered, it will cause a great threat to the environment. As an important part of the waste lead storage pool, the lead paste is an important part of the waste lead storage pool, because its composition is complicated. In order to recover the key and difficult points, the traditional fire method has the advantages of high energy consumption, low lead recovery, lead dust and SO2, which are serious to the environment. And the wet process technology has attracted more and more attention due to the advantages of high direct metal yield and low pollution. The organic matter treatment system has become an important research with its low pollution advantages. The paper firstly uses two reductant FeSO_4 and Na_2SO_3 to reduce and transform PbO_2, and uses two kinds of desulfurizer, NaOH and Na_2CO_3 to remove PbSO_4. Secondly, the leaching behavior of the main component PbO_2 and PbSO_4 in the alkaline xylitol system is investigated, and the leaching behavior of the lead paste in the alkaline xylitol system is also carried out. At last, the electrodeposition process of alkaline xylitol and lead solution was preliminarily explored. By means of X ray diffraction (XRD), scanning electron microscopy (SEM) and energy spectrum (EDAX), the evolution of the phase of the insoluble substances and the composition and morphology of the insoluble compounds were analyzed. The Fourier transform infrared spectroscopy (FTIR) was used to analyze the change of the organic groups in the leaching solution. The main research results of the paper are as follows: the results of PbO_2 reduction show that the reduction effect of Na_2SO_3 is obviously better than that of FeSO_4.FeSO_4 reduction: FeSO_4 excess coefficient is 1~1.1, reaction time 90~120min, reaction temperature 90 C, and the molar ratio of H_2SO_4 to PbO_2 is 3:1, but the highest reduction rate of PbO_2 is only the best condition of 52.4%.Na_2SO_3 reduction. The Na_2SO_3 excess coefficient is 6, the reaction time is 90~120min, the reaction temperature is 90 C, the reduction rate of PbO_2 can reach 100%.PbSO_4, the result of desulfurization transformation experiment shows that the best condition of NaOH desulfurization is time 60~120min, temperature 90, and excess coefficient 1.4. The desulfurization rate is only the best condition of 88.88%.Na_2CO_3 desulphurization: time 60~90min, temperature 90 C, The excessive coefficient of 1.3, the desulfurization rate is only 80.61%. infrared spectrum analysis results show that in the alkaline xylitol solution, PbO_2 can oxidize the -OH in xylitol to -COO-, and in the solution and Pb in the form of metal organic compounds. The concentration of xylitol, NaOH concentration affects the PbO_2 leaching rate and the.PbO_2 leaching rate will follow the concentration of xylitol. The increase of the increase first and then decrease and then increase. The variation of xylitol concentration will lead to the different dissolution mechanism of PbO_2. The optimum conditions for the leaching of PbO_2 in alkaline xylitol system are NaOH concentration 1.5~2mol/L, the concentration of xylitol 0.53~0.79mol/L, the leaching temperature of 70, the leaching time 30~ 60min, and the leaching rate of PbO_2 to 99.18%.PbSO_4 in alkaline xylose The leaching study in the alcohol system showed that the concentration of xylitol and NaOH had the greatest influence on the dissolution of PbSO_4, and the time and temperature had little effect. When only xylitol components were found in the solution, PbSO_4 would not react with the reaction of.PbSO_4 in the alkaline xylitol system, which was performed under the co action of xylitol and NaOH in the alkaline xylitol. The optimum conditions of the system leaching are: reaction time 60~90min, reaction temperature 90 C, xylitol concentration 50~80g/L, NaOH concentration 60~80g/L, the leaching rate of PbSO_4 can reach 100%. direct leaching of alkaline xylitol system, and the best condition of lead extract leaching is obtained: reaction time 30~60min, reaction temperature 90, xylitol 80~120g/ L, the leaching rate of NaOH concentration 60~80g/L. plaster in alkaline xylitol system can reach 96.24%. Under this system, the short process leaching of lead paste can be realized. Preliminary study on electrodeposition of lead containing solution of alkaline xylitol system found that when the current density is 140A/m~2, the temperature is 40, NaOH concentration 100g/L, the concentration of xylitol 120g/L, and the solution lead concentration 100g/L, At the extreme distance of 4cm and the electrolyte circulation rate of 15m L/min, the current efficiency can reach 99.68% and the energy consumption of the cathode is 381.71k Wh/t. The surface of the cathode lead is relatively flat and the dendrite is less.
【學(xué)位授予單位】：河南科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：X705;TF812
本文編號(hào)：2172124
[Abstract]:The demand for lead is increasing in human society, but the mineral resources of lead concentrate are decreasing. Therefore, the recycling of lead has become an important way for the sustainable development of lead industry. At the same time, if the waste lead battery is not reasonably recovered, it will cause a great threat to the environment. As an important part of the waste lead storage pool, the lead paste is an important part of the waste lead storage pool, because its composition is complicated. In order to recover the key and difficult points, the traditional fire method has the advantages of high energy consumption, low lead recovery, lead dust and SO2, which are serious to the environment. And the wet process technology has attracted more and more attention due to the advantages of high direct metal yield and low pollution. The organic matter treatment system has become an important research with its low pollution advantages. The paper firstly uses two reductant FeSO_4 and Na_2SO_3 to reduce and transform PbO_2, and uses two kinds of desulfurizer, NaOH and Na_2CO_3 to remove PbSO_4. Secondly, the leaching behavior of the main component PbO_2 and PbSO_4 in the alkaline xylitol system is investigated, and the leaching behavior of the lead paste in the alkaline xylitol system is also carried out. At last, the electrodeposition process of alkaline xylitol and lead solution was preliminarily explored. By means of X ray diffraction (XRD), scanning electron microscopy (SEM) and energy spectrum (EDAX), the evolution of the phase of the insoluble substances and the composition and morphology of the insoluble compounds were analyzed. The Fourier transform infrared spectroscopy (FTIR) was used to analyze the change of the organic groups in the leaching solution. The main research results of the paper are as follows: the results of PbO_2 reduction show that the reduction effect of Na_2SO_3 is obviously better than that of FeSO_4.FeSO_4 reduction: FeSO_4 excess coefficient is 1~1.1, reaction time 90~120min, reaction temperature 90 C, and the molar ratio of H_2SO_4 to PbO_2 is 3:1, but the highest reduction rate of PbO_2 is only the best condition of 52.4%.Na_2SO_3 reduction. The Na_2SO_3 excess coefficient is 6, the reaction time is 90~120min, the reaction temperature is 90 C, the reduction rate of PbO_2 can reach 100%.PbSO_4, the result of desulfurization transformation experiment shows that the best condition of NaOH desulfurization is time 60~120min, temperature 90, and excess coefficient 1.4. The desulfurization rate is only the best condition of 88.88%.Na_2CO_3 desulphurization: time 60~90min, temperature 90 C, The excessive coefficient of 1.3, the desulfurization rate is only 80.61%. infrared spectrum analysis results show that in the alkaline xylitol solution, PbO_2 can oxidize the -OH in xylitol to -COO-, and in the solution and Pb in the form of metal organic compounds. The concentration of xylitol, NaOH concentration affects the PbO_2 leaching rate and the.PbO_2 leaching rate will follow the concentration of xylitol. The increase of the increase first and then decrease and then increase. The variation of xylitol concentration will lead to the different dissolution mechanism of PbO_2. The optimum conditions for the leaching of PbO_2 in alkaline xylitol system are NaOH concentration 1.5~2mol/L, the concentration of xylitol 0.53~0.79mol/L, the leaching temperature of 70, the leaching time 30~ 60min, and the leaching rate of PbO_2 to 99.18%.PbSO_4 in alkaline xylose The leaching study in the alcohol system showed that the concentration of xylitol and NaOH had the greatest influence on the dissolution of PbSO_4, and the time and temperature had little effect. When only xylitol components were found in the solution, PbSO_4 would not react with the reaction of.PbSO_4 in the alkaline xylitol system, which was performed under the co action of xylitol and NaOH in the alkaline xylitol. The optimum conditions of the system leaching are: reaction time 60~90min, reaction temperature 90 C, xylitol concentration 50~80g/L, NaOH concentration 60~80g/L, the leaching rate of PbSO_4 can reach 100%. direct leaching of alkaline xylitol system, and the best condition of lead extract leaching is obtained: reaction time 30~60min, reaction temperature 90, xylitol 80~120g/ L, the leaching rate of NaOH concentration 60~80g/L. plaster in alkaline xylitol system can reach 96.24%. Under this system, the short process leaching of lead paste can be realized. Preliminary study on electrodeposition of lead containing solution of alkaline xylitol system found that when the current density is 140A/m~2, the temperature is 40, NaOH concentration 100g/L, the concentration of xylitol 120g/L, and the solution lead concentration 100g/L, At the extreme distance of 4cm and the electrolyte circulation rate of 15m L/min, the current efficiency can reach 99.68% and the energy consumption of the cathode is 381.71k Wh/t. The surface of the cathode lead is relatively flat and the dendrite is less.
【學(xué)位授予單位】：河南科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：X705;TF812
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